HPCE法同时测定蒲公英中的四种组分

建立了高效毛细管电泳(HPCE)同时测定蒲公英中黄酮类化合物、咖啡酸和绿原酸的方法.在优化条件下,4种组分在10min内得到良好分离.绿原酸,异槲皮甙,槲皮素,咖啡酸的线性浓度范围分别为0.003～0.2,0.003～0.2,0.001～0.1,0.001～0.1mg/mL,线性相关系数分别为0.9999、0.9999、0.9998和0.9994.4种组分基于迁移时间和峰高的相对标准偏差分别为0.19%、0.34%、0.20%、0.23%和1.8%、2.6%、2.8%、2.7%.检出限分别为0.56、0.56、0.20和0.21μg/mL.方法可用于中国传统医学中的药物分析.     

毛细管电泳紫外检测法测定莲须中的槲皮素、木犀草素、山萘酚、异槲皮甙

采用毛细管区带电泳紫外检测法(CZE-UV)同时测定中药莲须中槲皮素、木犀草素、山萘酚、异槲皮甙4种有效成分.研究了缓冲溶液的离子浓度、pH值和电压对分离度和迁移时间的影响,得到了最佳分离实验条件.在离子浓度为40 mmol/L Na2B4O7缓冲溶液(pH 9.0)中,分离电压为16 kV,波长为254 nm时,槲皮素、木犀草素、山萘酚、异槲皮甙4种物质在10 min内得到了良好的分离测定,其检出限分别为5.0、6.7、4.5和6.0 mg/L.本方法应用于实际样品的测定,结果令人满意.     

毛细管区带电泳法测定芹菜素木犀草素和异槲皮甙

建立了毛细管区带电泳法(CZE)分析测定芹菜素、木犀草素和异槲皮甙的方法。研究了缓冲溶液的浓度、pH、分离电压等对分离的影响。在优化条件下,三种被测物质可以在11min内实现良好的分离。芹菜素、木犀草素和异槲皮甙的峰面积与浓度分别在0.001250~0.8000,0.002500~0.1000和0.002500~0.1000g.L-1浓度范围内呈良好的线性,线性相关系数分别为0.9995,0.9995和0.9981。检出限(S/N=3)分别为0.00042,0.0005和0.00082g.L-1。并对银菊珍珠胶囊中的芹菜素、木犀草素和异槲皮甙进行了测定,结果满意。     

高效液相色谱-分段检测法同时测定烟草中14种多酚类化合物

利用高效液相色谱-二极管阵列检测器(HPLC-DAD),建立了同时分析烟草中新绿原酸、绿原酸、隐绿原酸、东莨菪苷、咖啡酸、七叶亭、对香豆酸、阿魏酸、莨菪亭、7-羟基香豆素、芦丁、槲皮苷、山奈酚-3-O-芸香糖苷和槲皮素14种多酚化合物的方法。称取0.02 g烟末,加入5 mL 50%甲醇,超声萃取30 min,取上清液过水相滤膜后,采用Agilent SB-C18柱(3.0 mm×150 mm,1.8μm)进行分离,以0.05 mol/L磷酸二氢钾水溶液和甲醇为流动相,采用分段式检测,获得14种多酚类化合物在各自最佳检测波长下的信号,实现了良好分离。结果表明,14种多酚类化合物的色谱峰面积与其质量浓度呈良好的线性关系,相关系数r2>0.9997,检出限为0.01~0.15μg/mL,定量下限为0.03~0.50μg/mL,日内相对标准偏差(RSD)为0.70%~3.6%,日间RSD为4.0%~6.4%,加标回收率为95.2%~109%。该方法具有良好的灵敏度、精密度和回收率,适合于烟草样品中多种多酚类化合物的同时测定。     

磺丁基醚-β-环糊精手性流动相添加剂法拆分佐匹克隆对映体

采用磺丁基醚-β-环糊精(SBE-β-CD)为手性流动相添加剂,建立了反相高效液相色谱手性流动相添加剂法拆分分离佐匹克隆对映体的方法。在普通C18色谱柱(250 mm×4.6 mm×5.0μm)上,考察了水相pH、磺丁基醚-β-环糊精浓度、磷酸盐缓冲液浓度、甲醇含量、柱温等对佐匹克隆对映体拆分效果的影响。确定最适用的色谱条件:流动相为水相(5 mmol/L NaH2PO4,含磺丁基醚-β-环糊精5 mmo/L,以H3PO4调pH为3):甲醇=78:22(V/V),检测波长305nm,流速为1 mL/min,柱温为30℃,此条件下佐匹克隆对映体的保留时间分别为23.0和25.6 min,分离度为1.81。两对对映体质量浓度在0.04~0.36g/L范围内线性关系良好(r≥0.9990),保留时间的RSD分别为0.73%和0.80%,峰面积的RSD分别为1.2%和1.1%。     

高效毛细管电泳法同时检测苹果中4种多酚类化合物

利用高效毛细管电泳法(HPCE),对苹果中根皮苷,表儿茶素,芦丁,绿原酸4种多酚类化合物进行分离与测定。在最佳实验条件:缓冲溶液为10 mmol/L Na_2B_4O_7-H_3BO_3,pH 9.2,检测波长280 nm,分离电压25 kV,测定了4种多酚类化合物的标准品,其线性范围分别为0.005~0.120,0.005~0.550,0.004~0.450,0.020~0.600 mg/mL,相关系数r在0.9977~0.9992之间,检出限分别为34.1,56.7,37.8,38.9μg/L(S/N=3)。日内及日间精密度和平均回收率范围分别为0.13%~4.5%和为96.7%~104.5%,相对标准偏差(RSD)≤3.7%(n=3)。方法可用于苹果中多种酚类物质的同时检测。     

毛细管电泳法测定复方鱼腥草片中的绿原酸和槲皮素

建立了毛细管电泳法分析复方鱼腥草片中绿原酸和槲皮素的方法,通过研究缓冲溶液酸度和浓度、工作电压和进样时间的影响优化了分析条件。在优化的条件下,15min内实现了两种分析物质的良好分离。绿原酸和槲皮素峰高和质量浓度分别在0．05～0．80g／L和0．05～1．00g／L范围内成良好线性。基于迁移时间和峰高的重复性(RSD)分别为：绿原酸,1．91％和4．32％;槲皮素,2．30％和3．18％。绿原酸和槲皮素的检出限(S／N=3)分别为0．014g／L和0．015g／L。通过分析实际样品并做加样回收实验进一步验证了该方法的可行性。     

毛细管电泳电致化学发光法同时测定氯丙嗪、异丙嗪及其主要代谢物

建立了同时检测氯丙嗪、异丙嗪及其主要代谢物的毛细管电泳电致化学发光新方法。最佳实验条件为: 检测电位1.20 V,钌联吡啶浓度5 mmol/L,检测池磷酸缓冲溶液40 mmol/L (pH 6.5),分离磷酸缓冲溶液18 mmol/L (pH 4.8),进样电压11 kV,进样时间8 s,分离电压13.5 kV。方法的检出限(3σ)分别为氯丙嗪8.3×10~7 g/L、异丙嗪7.2×10~6 g/L、氯丙嗪亚砜1.9×10~5g/L和异丙嗪亚砜3.7×10~6g/L,各组分的电化学发光强度和迁移时间的相对标准偏差(RSD)分别不超过3%和1%。本方法具有简便、快速、灵敏、进样量少和不受共存物干扰等特点,可在不必预分离的情况下直接同时连续测定家犬尿样中的氯丙嗪、异丙嗪、氯丙嗪亚砜和异丙嗪亚砜。     

杜仲及其保健品中生物活性成分的毛细管电泳/电化学检测

采用毛细管电泳/电化学检测法(CE/ED)同时分离测定了杜仲叶、杜仲皮及市售杜仲保健品中芦丁、抗坏血酸、金丝桃甙、绿原酸、槲皮素等多种生物活性成分的含量,考察了运行缓冲液酸度和浓度、分离电压、氧化电位和进样时间等实验参数对分离、检测的影响。在最优化条件下,以300μm碳圆盘电极为检测电极,检测电位为 950 mV(vs.SCE),50 mmol/L硼砂的运行缓冲液(pH9.0)中,上述各组分在20 min内可基本实现基线分离。各组分浓度与峰电流在3个数量级范围内呈良好线性,检出限(S/N=3)在3.3×10-5~9.6×10-5g/L范围。该方法已成功地应用于杜仲及其保健品中生物活性成分的测定,结果令人满意。     

毛细管电泳-电化学检测法测定淮山中薯蓣皂苷和腺苷含量

建立了毛细管电泳-电化学检测(CE-ED)法测定淮山中薯蓣皂苷和腺苷的含量。考察了检测电位、运行缓冲液浓度和pH、分离电压及进样时间等的影响。在优化的实验条件下,对0.1mg/L薯蓣皂苷、腺苷在9min内实现了分离,其线性范围分别为0.1~1 000μg/L和0.1~1 200μg/L;检出限分别为0.04μg/L和0.03μg/L,峰电流的相对标准偏差(RSD,n=6)分别为1.7%、1.5%,迁移时间的RSD分别为0.7%、0.6%。该方法已用于淮山样品中薯蓣皂苷和腺苷的测定,样品加标回收率在98.0%~102.5%之间,RSD≤2.3%。     

多环芳二酐型聚酯亚胺膜的透气性能

多环芳二酐型聚酯亚胺膜的透气性能李悦生，丁孟贤，徐纪平（浙江大学高分子科学与工程研究所，杭州，３１００２７）（中国科学院长春应用化学研究所）关键词聚醚酰亚胺，聚酯酰亚胺，膜，透气性通常的聚酰亚胺加工性能较差，在芳环二酐的苯环间引入醚键等柔性基团后，其...     

Determination and study on residue and dissipation of benazolin-ethyl and quizalofop-p-ethyl in rape and soil

A QuEChERS (quick, easy, cheap, effective, rugged, and safe) method for the determination of benazolin-ethyl and quizalofop-p-ethyl in rape and soil by high-performance liquid chromatography-tandem mass spectrometry has been developed in this study. The residue and dissipation of benazolin-ethyl and quizalofop-p-ethyl in rape and soil were determined with the developed method. The half-lives of benazolin-ethyl in rape straw and soil were 3.7–5.1 days and 14.3–26.3 days, respectively. The half-lives of quizalofop-p-ethyl in rape straw and soil were 5.0-6.1 days and 0.3–9.7 days, respectively. The residue of benazolin-ethyl and quizalofop-p-ethyl in rapeseed and soil were below the detection limit (i.e., 0.5?mg?kg^?1, the maximum residue level of European Union for quizalofop-p-ethyl).     

微量元素与疾病诊断治疗的研究现状及展望

对国内外微量元素与疾病的关系及其诊断治疗的研究现状及研究动向进行了综述，包括：微量元素与地方病、癌肿、心血管病、糖尿病、眼病、神经系统病等。参考文献72篇。     

Ferrocene and ferrocenium modified clays and their styrene and EVA composites

In this work, ferrocene- and ferrocenium-containing salts were employed to modify montmorillonite. X-ray measurements show an increase in the interlayer spacing upon clay modification, which means that the larger and more organophilic cations were inserted into the gallery space of montmorillonite. Attempts to prepare nanocomposites of polystyrene and ethylene vinyl acetate copolymers lead to immiscible systems; the morphology of these systems was elucidated with TEM, XRD and cone calorimetry. The thermal stability of the composites is greater than that of the virgin polymer.     

Ti-V基储氢合金及其氢化物的物相结构与组分优化设计

Ti-V基储氢合金在室温、常压下即可表现出良好的储氢特性,且质量储氢容量明显高于传统AB₅型储氢合金,从而在氢气的精制和回收、运输和储存及热泵等方面有较早的应用。 此外,在混合气体分离、核反应堆中处理氢的同位素、镍氢电池及燃料电池负极材料等方面也得到了广泛的研究与关注。 基于目前Ti-V基储氢合金的研究现状,概述了该类合金的优势、限制性因素(包括成因)及改性手段。 此外,为了进一步理解Ti-V基合金储氢机理、构建合金组分与储氢特性之间的对应关系,本工作重点围绕Ti-V基储氢合金及其氢化物的结构、组分优化设计展开综述,并对其未来研究方向做出展望。     

钒与糖代谢及糖尿病

微量元素钒作为生物体内必需元素，经证实有很重要的生理学功能，与机体糖代谢有十分密切的关系，且能降低糖尿病动物模型的高血糖，极有可能被开发为治疗糖尿病的药物。     

Synthesis and Optical and Redox Properties of Symmetric and Asymmetric BODIPYs

Herein, we present the synthetic route and the photophysical, electrochemical as well as laser properties of novel red‐emitting boron‐dipyrromethenes (BODIPYs) bearing arylethyne moieties. Such functionality is added along the main axis of the chromophore leading to single‐ and double‐substituted derivatives. The relationship between the dye structure and the lasing properties is studied in detail with the help of the photophysical and electrochemical properties as well as quantum mechanical simulations. The asymmetric substitution of the parent dye induces inhomogeneities in the charge distribution, which leads to an overall loss of the fluorescence capacity, mainly in polar media. Such non‐radiative deactivation processes can be softened by decreasing the electron‐donor ability of the substituent or even avoided by symmetrical substitution. Thus, grafting of the arylethyne moieties at the longitudinal axis of the indacene core results in an effective strategy to develop red‐edge BODIPYs with highly efficient and photostable laser emission.     

Conformations and steric and stacking interactions of trisubstituted ureas and thioureas with alkyl and phenyl groups

The monomeric ν(N—H) vibrations of various trisubstituted ureas of the R₂UPh type and -thioureas of the R₂TUPh type have been studied. The trans—out isomerism in the former and the trans—out—cis isomerism in the latter are discussed from the point of view of steric effect. The monomeric ν(N—H) vibrations of RPhUPh and RPhTUPh are also examined. The single band appearing in the spectrum of both ureas is characteristic of the cis form; this suggests the existence of phenyl—phenyl interaction (the stacking interaction proposed by Galabov et al. [10]). Behavior of ν(N—H) vibrations at several concentrations is shown to be clearly different in the three forms (trans, out and cis). The presence of the cis form is confirmed by solvent effect experiments.     

含茂基苯并三氮唑基镧系有机配合物的合成及表征

三茂基镧系化合物和苯并三氮唑在四氢呋喃中反应,合成了7个未见文献报道的含茂基苯并三氮唑基镧系有机配合物,经元素分析、IR和MS测定,从有关数据推测了这类配合物的可能结构。